HPLC-ICP-MS测定富硒芦笋中硒代蛋氨酸的不确定度评定

Uncertainty Evaluation of Determination of Selenomethionine in Selenium-Enriched Asparagus officinalis L. by HPLC-ICP-MS

目的:对高效液相色谱-电感耦合等离子体质谱法测定富硒芦笋中硒代蛋氨酸含量的不确定度进行分析评定。方法:按照行业标准《粮谷中硒代半胱氨酸和硒代蛋氨酸的测定液相色谱-电感耦合等离子体质谱法》(NY/T 3556—2020)对富硒芦笋中硒代蛋氨酸的含量进行检测,依据《测量不确定度评定和表示》(GB/T 27418—2017)和《化学分析中测量不确定度评估指南》(RB/T 030—2020)对引入的各类不确定度分量进行分类,通过构建数学模型精确评价测定过程中的测量不确定度。结果:当富硒芦笋中硒代蛋氨酸含量为0.558 mg·kg^(-1)时,在95%的置信区间下,扩展不确定度为0.034 mg·kg^(-1)(k=2)。影响检测结果不确定度的主要因素为试样提取回收率、标准溶液配制和标准曲线拟合。结论:在测定过程中,应保证标液和器具质量,并严格按照标准化流程操作,以降低测量不确定度,获得更加准确的测量结果。

Objective:To evaluate the uncertainty of selenomethionine content in selenium-enriched Asparagus officinalis L.by high performance liquid chromatography-inductively coupled plasma mass spectrometry.Method:The selenomethionine content of selenomethionine in selenium-enriched Asparagus officinalis L.was detected according to industry standard NY/T 3556—2020,and various uncertainty components were classified according to GB/T 27418—2017 and RB/T 030—2020,and the measurement uncertainty in the determination process was accurately evaluated by constructing mathematical models.Result:When the selenomethionine content of selenomethionine in selenium-enriched Asparagus officinalis L.was 0.558 mg·kg^(-1),the extended uncertainty was 0.034 mg·kg^(-1)(k=2)with 95%confidence interval.The main sources affecting the uncertainty of test results are the recovery rate of sample extraction,standard solution preparation and standard curve fitting.Conclusion:In the measurement process,the quality of the standard liquid and instruments should be guaranteed and the standardized procedures should be strictly followed to reduce the measurement uncertainty and obtain more accurate measurement results.